CHAPTER ONE

1.0 INTRODUCTION

1.1 THE OVERVIEW OF SIWES PROGRAMME

The Student Industrial Work Experience Scheme (SIWES) is an accepted skills

programme which forms part of the approved academic standards in the degree

programme for Nigerian Universities. In 1974, the Federal Government of Nigeria

introduced the national policy on Industrial training, called the Students,

Industrial Work Experience Scheme (SIWES). This programme is under the

umbrella of the Ministry of Education through the Industrial Training Fund (ITF),

was designed to help students acquire the necessary practical

education/experience in their fields of study and other related professions.

This is an effort which was created in order to bridge the existing gap between

the theory taught in the classroom and practice of science, agriculture, medicine,

engineering, technology and other professional programmes in the Nigerian tertiary

institutions. This programme is aimed at exposing the students to the use of

various machines and equipment’s, professional work methods and ways of

safeguarding the work areas in industries as well as other organizations and

parastatals. The programme was established basically to impact elaborate practical

understanding to students with respect to their various disciplines. It is also

intended that the student through a process of relation to academic knowledge and

practical industrial application would understand the underlying principl es and

become better focused and acquire the practical applications towards excellence in

his or her discipline.

1
The Students Industrial Work Experience Scheme (SIWES) programme involves

the student, the Universities and the industries. This training is funded by the

Federal Government of Nigeria and jointly coordinated by the Industrial Training

Fund (ITF) and the National Universities Commission (NUC).

Industrial training fund in its policy statement No.1, published in 1973, inserted a

clause dealing with the issue of practical skills among locally trained professionals.

Section 15 of the policy statement states inter-alia, that “Great emphasis will be

placed on assisting certain products of post-secondary school system to adopt or

orientate easily to their possible post graduate job environment. The scheme

exposes students to industry based skills necessary for a smooth transition from

classroom to the world of work. It affords student of tertiary institutions the

opportunity of being familiarized exposed to the needed experience in handling

machinery and equipment which are not available in the education institute.

1.2 AIM AND OBJECTIVES OF STUDENT WORK INDUSTRIAL

EXPERIENCE SCHEME (SIWES)

The aim and objectives of the SIWES are as follows:

 To prepare students for the work situation they are likely to meet after

graduation

 To provide students with an opportunity to apply their theoretical

knowledge in real work situation, thereby bridging the gap between

university work and actual practices.

 To expose students to work methods and techniques in handling the

equipment and machinery that may be available in universities

2
  Provision of avenue for students in Nigerian universities to gain industrial

skills and experience in their course of study.

 To enlist and strengthen employers involvement in entire educational

process of preparing university graduate for employment.

1.3 IMPORTANCE OF SIWES

SIWES have a lot of importance attached to it which includes:

 It helps to improve the quality of skilled manpower of the students. The

scheme provides a forum for industries to evaluate prospective employers

and gives feedback to institutions

 The scheme gives students practical knowledge of course of study

 SIWES program exposes students to real life situation, thus supplementing

the theoretical lesson

 SIWES program establish a close collaboration between institutions and

industries, a factor which is essential for preparing people for the

workforce

1.4 INDUSTRIAL TRAINING FUND (ITF)

The ITF has an aim in those establishments that handles the SIWES programme.

Its responsibilities performed through this arm involve formulating policies and

guidelines on SIWES for dissemination to bodies participating in the SIWES

programme through;

 Regularly organizing orientation programmes for students prior to their

attachment.

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  Receiving and processing master lists and placement lists forwarded from

the institutions.

 Supervising students on industrial attachment.

 Providing logistics and materials necessary for effective administration of

the scheme.

 Providing information on companies for attachment and assisting in the

industrial placement of students.

 Ensuring the visitation of ITF officers to the supervising agencies,

institutions, employers and students on attachment.

 Continuously receiving and carrying out research into the operations of

SIWES

1.5 DESCRIPTION OF THE ORGANIZATION

The Nigerian National Petroleum Corporation, Research and Development (R&D)

Division

1.5.1 Historical Background

The (NNPC, R&D) Division was established in 1977 to solve the operational and

technical problems of the oil and gas industry through the application of the

results of scientific research and the development of technology. R&D has highly

qualified personnel and experienced engineers.

Research and Development Division (R&D) is a Corporate Service Unit (CSU) of the

Nigerian National Petroleum Corporation (NNPC) is situated in Port at NNPC EPCL

Life Camp Complex, P.M.B. 5373, Eleme.

The division renders Research and Laboratory Services to the Oil and Gas

Industries.

4
NNPC, R&D business entails the provision of Research Initiatives; Technology

Development and Commercial Laboratory services to the Oil and Gas Industries.

NNPC, R&D Quality Management System covers all requirements of NIS ISO

9001:2008 excluding the design requirements in 7.3.

1.5.2 RESEARCH AND DEVELOPMENT MANAGEMENT STRUCTURE

The R&D is staffed with highly professional and skilled personnel with considerable

experience in research and laboratory services to the oil and gas industries.

Below is the Division’s organogram, depicting the administrative structure of the

company. The Group General Manager (GGM) is the Chief Executive Director of the

Division. He is supported by three general managers, one in charge of Refining and

Petrochemicals (R&P) Department, the second one in charge of Exploration and

Petroleum Engineering (E&P) Department and the third one in charge of Support

and Services (S&S) Department. The Refining and Petrochemicals Department is

made up of Petroleum Product Research and Services, Environmental Research and

Services, Analytical Services, Process and Catalysis and Chromatography sections;

Exploration and Petroleum Engineering Department is made up of Exploration

Research and services, Petroleum Engineering Research and Services, Pressure

Volume and Temperature (PVT) and Renewable Energy Research and Services and;

Support and Service Department is made up of Human Resources/Administrative,

Technical Services, Finance and Accounting and Protocol sections.

In addition, there is a Managing Director’s Division made up, Planning and Business

Development, Health Safety and Environment, Internal Audit, Collaborative

Research and the Company Secretariat and Legal Advisory Services departments.

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 All the departments are supported by Sectional and Units heads. The total staff

strength is about 500.

Group General Manager

Research and Development

GGM’S Office Audit

Planning and Business Development Collaborative Research

Health Safety and Environment Legal

General Manager General Manager General Manager

Refining and Petrochemicals Exploration and Petroleum Support Services

Fig. 1.0 R&D Organizational Chart

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1.5.3 Vision and Mission of Research and Development (R&D)

Visions:

Nigerian National Petroleum Corporation, Research and Development Division will

be a world class petroleum research centre, driven by innovation and quality.

Mission:

Nigerian National Petroleum Corporation, Research and Development Division

carries out research, develops technology and provide laboratory services in the oil

and gas industry.

1.5.4 R&D Quality Policy Statement

Research and Development shall strive to sustain high quality delivery in carrying

out research, developing technology and providing services to the oil and gas

industry. To this end, research and development shall implement and maintain

effective quality systems based on NIS: ISO 9001: 2008 that will meet regulatory

and legal requirements as well as ensure continual improvement to meet and exceed

our customers’ expectation.

1.5.5 R&D Quality Objectives

 To meet the customers’ needs for precision accuracy sensitivity and specificity

in line with the statutory requirements of ISO 9001:2008 (Clause 8:2.1)

 To meet the commercial performance criteria, namely: timeliness and

competitive cost by efficient utilization of technological, human and material

resources.

 To make cost-effective use of the technology financial human and material

resources to provide quality services that meet customers’ expectations.

7
 CHAPTER TWO

NIGERIAN NATIONAL PETROLEUM CORPORATION, RESEARCH AND

DEVELOPMENT (R&D) DIVISION’S CORE BUSINESS

2.1 CRUDE OIL ASSAY

A crude oil assay is the chemical evaluation of crude

oil feedstock by petroleum testing laboratories. Each crude oil type has

unique molecular and chemical characteristics. No two crude oil types are identical

and there are crucial differences in crude oil quality. The results of crude oil assay

testing provide extensive detailed hydrocarbon analysis data for refiners, oil

traders and producers. Assay data help refineries determine if a crude oil

feedstock is compatible for a particular petroleum refinery or if the crude oil

could cause yield, quality, production, environmental and other problems.

The assay can be an inspection assay or comprehensive assay. Testing can include

characterization of the whole crude oil and the various boiling

range fractions produced from physical or simulated distillation by various

procedures. Information obtained from the petroleum assay is used for detailed

refinery engineering and client marketing purposes. Feedstock assay data are an

important tool in the refining process.

Below are the summary of the sections that carry out crude oil assay in the

Nigerian National Petroleum Corporation, Research and Development Division.

i. Petroleum Product Research and Development

 Determination of yield and distillate parameters for accurate evaluation of

price potentials of crude in the international market.

 Determination of the True Boiling Point (TBP) curve of crude oil.

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  Evaluation of crude oil for product state changes and refinery product

optimization

ii. ANS: Petroleum Products Quality Testing (PPQT)

 Whole crude characterization from well heads/flow stations (Physico-

chemical analysis)

 Crude Oil Assay (Physio-Chemical Characterization)

 Product Identification and Quality Assessment of petroleum products

 Crude Oil Finger Printing for identification

iii. Spectroscopy and Elemental Analysis (SEAL)

 Metal analysis for Crude Oil assay

 Elemental analysis (CHN&O) in petroleum and its products (no CHN Analyzer

available)

 Metal analysis in petroleum and its products

 Metal Analysis in Biological samples

iv. Water & Specialty Chemicals (WASC)

 Effluent/waste water evaluation for performance monitoring/regulatory

purposes

 Quality characterization of boiler/cooling (process) water for refineries.

 Chemical analysis for Water Potability Test.

 Water Compatibility Studies for water re-injection operations.

v. Chromatography

 Crude characterisation

 Determination of the boiling range distribution of distillate fractions

 Analysis of Overhead Gas Associates and Non- associates gases

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  Determination of Polynuclear Aromatic Hydrocarbon (PAH) by HPLC using

PDA detector in waste water, sediments and soil for environmental studies.

 Determination of Total Petroleum Hydrocarbon (TPH) in soil and water.

vi. Environmental Research and Service

 Air Quality Monitoring

 Noise pollution monitoring

 Radiation Monitoring

 Thermal monitoring

 Air Pollution Modelling

 Air Dispersion Modelling and Monitoring

 Climate Change Analysis

 Quality Test on petroleum products

vii. Process and Catalysis

 Process analysis (material and energy balance studies) of refinery and

petrochemical processes

 Process modelling and simulation of refinery and petrochemical processes

 Process integration studies and optimization of energy usage (Pinch

Analysis)

 Process optimization (linear programming) of refinery and petrochemical

processes

 Analysis, modelling and simulation of processes involved in oil and gas

production (e.g., separation of oil/gas/sand mixture, gas purification, etc.)

 Flow assurance studies of multiphase flow in pipelines and flow terminal

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2.2 LABORATORY CRUDE OIL ASSAY

Laboratory assays of crud oil and condensate are conducted to establish yield

(weight % / volume %) and the product physical/chemical properties. This is by

distillation up to 3500c using a 15 plate theoretical column and from 350 0c to

450+0c by high vacuum flash distillation using AUTOMAXX 9100. The Assay

results give a useful and detailed picture of the quality of oil. Yield from the

original crude oil is measured as % vol or % wt.

Light ends analyse (C 1 – C5), and individual fractions are separated and tested.

Individual cuts of butanes and lighter components, light Naphtha, heavy Naphtha,

kerosene, light distillate, gas oils, vacuum gas oil, light & heavy residues receive

extensive analyses for each fraction produced by the distillation process.

Analysis on crude oil and fraction includes:

 API Gravity, Correlation (calculation)

 Specific Gravity @60/60 0F, D5002

 Yield % volD664

 Water by distillation vol. %, D4006/D95

 Pour point 0c D97 D5853

 Kinematic Viscosity D445

 Water and sediment vol. %, D96 D4007

 Reid Vapour Pressure @100 0F, psi, D323

 Sulphur wt. %, D4294

 Hydrogen sulphide mg/k, UOP163

 Wax content wt.%, BP 237

 Copper mg/kg, D5863

 Acid Number mg KOH/g,

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 2.3 PROCEDURE FOR CRUDE OIL ASSAY

CRUDE OIL TREATMENT

Crude oil treatment is the process of treating and removing the unwanted element

or substance from crude to a bearable level. The chart below entails how the crude

oil is treated in the laboratory for crude Assay.

Sample received at
the laboratory

Refrigerate
sample to -50C

Water content test

Water content No Dewatering to

less than 0.3% less than 0.3%

Yes

Equipment preparation Determination of sample

and wash run ASTM D2892 Distillation
physical properties, charge
of crude petroleum
measured and loading
Collect the overhead gas
for analysis
Generation of
distillation cuts

Distillate Storage and ASTM 536 vacuum

characterization (Physico- Distillation for reduce
chemical Analysis) crude and residue

QA/QC Results Analysis

compilation and Delivery

Fig. 2.3.0 Flow chart for Crude Assay sample Handling and management procedure
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2.3.1 SAMPLE (CRUDE OIL) RECEIVED AT THE LABORATORY

The sample must be received in a sealed metallic container and should show no

evidence of leakage. Receive samples that meet the requirements of the sampling

procedure in accordance to practice D4057 or D4177

2.3.2 SAMPLE PRESERVATION

Cool the sample to a temperature between 0 0C and -50C by placing it in a

refrigerator for several hours (preferably overnight) before opening. For waxy or

too viscous sample, raise the temperature of sample to 5 0C above its pour point.

Agitate the sample by preferably shaking or other means that are appropriate to

its size, to ensure that it is well mixed.

Fig. 2.3.2.0 Sample Preservation Method

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2.3.3 WATER CONTENT TEST

This test method describes the laboratory determination of water and sediment in

crude oils by means of the centrifuge procedure. Knowing water content in

hydrocarbons enables clients to take steps to reduce risks from corrosion, safety

problems, and infrastructure damage which can be caused from unwanted water

content levels.

Significance: The water and sediment content of crude oil is significant because it

can cause corrosion of equipment and problems in processing. A determination of

water and sediment content is required to measure accurately net volumes of

actual oil in sales, taxation, exchanges, and custody transfers.

Summary of the test: Equal volumes of crude and water saturated hydrocarbon

(Toluene) are placed into a cone-shape centrifuge tube. After centrifugation, the

volume of the higher gravity water and sediment layer at the bottom of the tube is

read.

Procedure:

Fill each of two centrifuge tubes to the 50-mL mark with sample directly from the

sample container (crude oil). Using a pipette or other suitable volume transfer

device add 50 mL of toluene, which has been water saturated at 60°C (140°F) or

71°C (160°F) Read the top of the meniscus at both the 50 and 100-mL marks. Add

0.2 mL of demulsifier solution (ethelene oxide) to each tube, using a 0.2-mL pipet

or other suitable volume transfer device, such as an automatic pipettor.

Stopper the tube tightly and invert the tubes ten times to ensure that the oil and

solvent are uniformly mixed.

In the case where the crude oil is very viscous and mixing of the solvent with the

oil would be difficult, the solvent may be added to the centrifuge tube first to

14
facilitate mixing. Take care to not fill the centrifuge tube past the 100-mL mark

with the sample.

Loosen the stoppers slightly and immerse the tubes to the 100-mL mark for at

least 15 min in the bath maintained at 60 6 3°C (140 6 5°F). Secure the stoppers

and again invert the tubes ten times to ensure uniform mixing of oil and solvent.

(Warning—the vapor pressure at 60°C (140°F) is approximately double that at 40°C

(104°F).)

Place the tubes in the trunnion cups on opposite sides of the centrifuge to

establish a balanced condition. (If the tubes cannot be counter-balanced by eye,

place them, in their trunnion cups, on either side of a balance and equalize their

masses by the addition of water to the trunnion cups.) Retighten the corks and spin

for 10 min at a minimum relative centrifugal force.

Immediately after the centrifuge comes to rest, following the spin, read and

record the combined volume of water and sediment at the bottom of each tube, to

the nearest 0.05mL from 0.1 to 1mL graduations, and to the nearest 0.1mL above

1mL graduations. Below 0.1mL, estimate to the nearest 0.025mL

2.3.4 DEWATERING AND DESALTING

Crude oils are complex mixtures obtained from many parts of the world, and all

crudes contain dilute dispersion/emulsion of ultrafine water droplets containing a

variety of salts, solids and metals. These emulsions might be quite stable due to the

presence of natural surfactants in oil such as asphaltenes, resins, naphthenic acids,

fine solids, etc. Adverse effects of these impurities can result in shortened unit

run lengths and reduced equipment reliability. To prevent corrosion, pluggi ng,

fouling of equipment, electrical desalting plants are often installed in crude oil

production units in order to remove water-soluble salts from an oil stream. The

15
refiners often wash the crude oil with fresh water, add chemical (demulsifier), and

use electrical desalting vessel to remove the added water and most of the inorganic

contaminants from the crude oil.

Electrical Desalter is the typical method of crude-oil desalting. After separation

by gravity settling, crude oil can be desalted by following the steps:

• The crude oil is preheated to decrease its viscosity for easy separate water from

crud and hence easy desalt. Preheating also increases demulsifier reactivity, and

destabilizing emulsion, however, the crude temperature is limited to avoid its

vaporization in the desalter, and prevent damage to the electrical grid insulator

bushings.

• The chemicals (demulsifiers) used are surfactants which migrate to the oil/water

interface to rupture the stabilizing film around the water droplets and allows them

to merge and coalesce. Chemical usage rates vary widely with crude type, and

desalter equipment. Chemicals are more efficient with basic pH water, while

electrical desalters function much better in acid pH range. Low pH result in

excessive corrosion, while high pH permits NH4OH (added to increase pH) to

migrate into the crude. Excessively high pH can aid in stable emulsion formation; So

typical pH control will be required.

• Addition of fresh water (wash water), increase coalescence and destabilizing

emulsion. The volume of wash water can be fixed from 3 to 10%; its value is

governed by the refiner’s needs.

• Wash water mixing is applied to ensure that the added fresh water is dispersed

well so that it can be available to combine with the contaminants in the crude.

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Wash water mixing is accomplished by a mixing valve with adjustable pressure drop.

• Finally, the heavier water particles settled at the bottom while the lighter crude

floats on top. The two layers are then separated by draining (decantation).

Fig. 2.3.4.1 Dewatering Unit

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Fig. 2.3.4.2 flow diagram for desalting and dewatering

2.4 EQUIPMENT PREPARATION AND WASH RUN

This is the process of preparing the equipment (Automaxx 9100) for crude oil

distillation by carrying out simple distillation with TOLUENE to wash and clean the

vital parts of the equipment for proper crude assay result. This process is also use

to determine the condition of the equipment, whether it’s in good condition or in

bad condition.

2.5 ASTM DISTILLATION OF CRUDE OIL USING AUTOMAXX 9100

This distillation system is designed for the fully automatic distillation of crude oil

and petroleum products. Crude oil distillation can be complex and time consuming.

Our crude oil distillation system includes everything needed to perform the ASTM

methods, D2892 and D5236, for distilling crude oil. The system’s automation

minimizes the operator time needed to perform the test. The equipment design

makes the test straightforward and easier to perform.

18
Fig. 2.5.0 Automaxx 9100

Distillation is a chemical process where a mixture made of two or

more liquids (called "components") with different boiling points can be separated

from each other. The mixture is heated until one of the components boils (turns to

a vapor). The vapor is then fed into a condenser, which cools the vapor and changes

it back into a liquid that is called distillate. What remains in the original container

is called the "residue. In other word, distillation is a process by which a desired

product is separated from other component of feedstock by taking advantage of

the difference in the boiling points of the various components of the feedstock. As

the feedstock is heated, the boiling temperature of some of its lighter components

19
is reached. The lighter components are flashed-off as vapor from the heavier

components.

The concepts for crude oil distillation are primarily the same for both atmospheric

and vacuum distillation units. However, this section will only deal with the

fractionation tower of the atmospheric distillation unit. The degree of

fractionation in a crude oil distillation unit is measured by the temperature

difference between 95% vol. ASTM (American Standard Temperature and

Measurement) of the lighter product and 5% vol. ASTM of the adjacent heavier

product. These lighter products are composed kerosene and light gas oil. The

heavier products are composed of heavy gas oil and fuel oil. When the temperature

difference gives the 95% point of the lighter products to be less than the 5%

point of the heavier products, the difference in temperatures is referred to as an

ASTM gap. For the reverse case, the situation is referred to as an ASTM overlap.

Fractionation performance is at its best when there is an ASTM gap between the

products. As fractionation decreases, the gap becomes an overlap, a greater

number of the components of the two products are not separated. Fairly complete

fractionation may be expected in the upper regions of the fractionation tower

between lighter products such as kerosene and light gas oils. However, lower in the

fractionation column such separation is not possible. It may be pointed out, that in

the lower levels of the fractionation column, there is an ASTM overlap. During

crude oil distillation steam stripping is used to further remove the entrained l ight

end products from the draw of

products.

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2.5.1 ATMOSPHERIC DISTILLATION BY ASTM D2892

As the name implies, the pressure profile in atmospheric distillation unit is close to

the atmospheric pressure (760mmhg) with highest pressure at the bottom stage

which gradually drops down till the top stage of the column.

The purpose of atmospheric distillation is primary separation of various 'cuts' of

hydrocarbons namely, fuel gases, LPG, naphtha, kerosene, diesel and fuel oil.

The heavy hydrocarbon residue left at the bottom of the atmospheric distillation

column is sent to vacuum distillation column for further separation of hydrocarbons

under reduced pressure.

The temperature is highest at the bottom of the column which is constantly fed

with heat from bottoms reboiler. The reboiler vaporizes part of the bottom outlet

from the column and this vapor is recycled back to the distillation column and

travels to the top stage absorbing lighter hydrocarbons from the counter current

crude oil flow. The temperature at the top of the column is the lowest as the heat

at this stage of the column is absorbed by a condenser which condenses a fraction

of the vapors from column overhead. The condensed hydrocarbon liquid is recycled

back to the column. This condensed liquid flows down through the series of column

trays, flowing counter current to the hot vapors coming from bottom and

condensing some of those vapors along the way.

The Automaxx 9100 distillation column has 15 theoretical plates and complies fully

with ASTM D2892 and the packed column is configured to distill the crude oil at

atmospheric up to 3500C.

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The products of atmospheric distillation include:

 LPG and lighter gases

 Straight-run gasoline

 Naphtha

 Gas Oil

 Fuel Oil (kerosene)

 Atmospheric Residuum (bottoms/asphalt)

Fig. 2.5.1.0 Atmospheric distillation blog flow diagram

22
2.5.2 VACUUM DISTILLATION (ASTM 5236)

Crude oil is first refined in an Atmospheric Distillation Column. Fractions of crude

oil such as lighter gases (C1-C4), gasoline, naphtha, kerosene, fuel oil, diesel etc.

are separated in the atmospheric distillation column. The after taking out these

lighter hydrocarbon cuts, heavy residue remaining at the bottom of the

atmospheric distillation column needs to be refined. These heavy hydrocarbon

residues are sent to a Vacuum Distillation Column for further separation of

hydrocarbons under reduced pressure.

Fig. 2.5.2.0 Vacuum Distillation Unit

23
Heavies from the atmospheric distillation column are heated to approximately

400˚C in a fired heater and fed to the vacuum distillation column where they are

fractionated into light gas oil, heavy gas oil and vacuum reside. Some heavy

hydrocarbons cannot be boiled at the operating temperature and pressure

conditions in the atmospheric distillation column. Hence they exit the bottom of

the column in liquid state and are sent to the vacuum distillation column where they

can be boiled at a lower temperature when pressure is significantly reduced.

Absolute operating pressure in a Vacuum Tower can be reduced to 20 mm of Hg or

less (atmospheric pressure is 760 mm Hg). In addition, superheated steam is

injected with the feed and in the tower bottom to reduce hydrocarbon partial

pressure to 10 mm of mercury or less. Lower partial pressure of the hydrocarbons

makes it even more easier for them to be vaporized, thus consuming less heat

energy for the process.

A typical Process Flow Diagram (PFD) of such a vacuum distillation column is

presented in the figure below. Steam ejectors can be used to suck the lighter

hydrocarbon vapors at low pressure from the top of the column. These vapors are

then cooled down to condense the steam which had been introduced in the column

earlier. The condensed oily water is removed and can be recycled to the column

after boiling it. Hydrocarbon vapors are taken out at this stage.

Two different cuts of hydrocarbons - 'light vacuum gas oil' and 'heavy vacuum gas

oil' are separated in the vacuum distillation column at different stages of the

column, based on the difference between their boiling point ranges. The liquid

being drawn at low pressure needs to be pumped. Then it is heated and partially

recycled back to the column. Part of is taken out as vacuum distillation products -

24
'light vacuum gas oil' or 'heavy vacuum gas oil'. Light vacuum gas Oil is sent to a

hydrotreater and then to a 'catalytic cracking' unit to obtain smaller chain

hydrocarbons. Heavy vacuum gas oil is also sent for cracking using hydrogen in a

'hydrocracking unit' to produce smaller chain hydrocarbons.

Heavy hydrocarbons which cannot be boiled even under reduced pressure remain at

the bottom of the column and are pumped out as 'vacuum residue'. The vacuum

distillation column bottom residue can only be used for producing coke in a 'coker

unit' or to produce bitumen.

Fig. 2.5.2.1 Vacuum Distillation Flow Diagram

25
 2.5.3 CRUDE DISTILLATION FRACTIONS / CUTS

KEY:

IBP - Initial Boiling Point

>IPB0 C
OG
OG - Overhead Gas

SRG - Straight Run Gasoline

IBP-900 C SRG

90-1200 C LIGHT NAPHTHA

120-1700 C HEAVY NAPHTHA

170-3000 C KEROSENE

300-3500 C ATMOSPHERIC GAS OIL

350-4000 C LIGHT VACUUM GAS OIL

400-4500 C HEAVY VACUUM GAS OIL

450+0 C VACUUM RESIDUE

26
2.6 PHYSICO-CHEMICAL ANALYSIS OF THE FRACTIONS / CUTS

This is the analysis or test method carried out in the laboratory to determine the

following:

 Density and API gravity

 Specific gravity

 Reid vapor pressure

 Off – gasses

 Cloud point
 Pour Point

 Viscosity

 Aniline point

 Asphaltenes, carbon residue and asphalt content

 Flash point

 fire point

 Smoke point

 Copper corrosion test

 Colour

 Antiknock quality (octane number)

 Cetane number

 Carbon Hydrogen ratio

27
2.7 TEST METHOD FOR CRUDE PETROLEUM AND PETROLEUM

FRACTION/CUTS AND PROCEDURES

2.7.1 AMERICAN PETROLEUM INSTITUTE (API) GRAVITY TEST (ASTM

D1298)

API Gravity is the factor governing the quality of crude oils. However, the API

gravity of petroleum product is an uncertain indication of its quality.

API can also be determined by the following correlation:

API gravity = 141.5 - 131.5

SP. Gravity @ 15.6/15.60 C

This test is based on the principle that the gravity of a liquid varies directly

with depth of immersion of a body floating in it. The floating body which is

graduated by API gravity units in this method, is called API Hydrometer. The

API gravity is read by observing the freely floating API Hydrometer and noting

the graduation nearest to apparent intersection horizontal plane surface of the

liquid with the vertical scales of the hydrometer, after temperature equilibrium

have been reached. The temperature of the sample is read from separate

accurate ASTM thermometer in the sample from a thermometer which is an

integral part of the hydrometer (Thermo-hydrometer).

<

2.7.2 SMOKE POINT TEST (ASTM D1322)

Smoke point is the maximum height in millimeters of a smokeless flame of fuel

burned in a wick-fed lamp in specified design.

28
 Fig. 2.7.2.0 Smoke Point Tester (Lamp)

Significance of the test:

This test method provides an indication of the relative smoke producing properties

of kerosene and aviation turbine fuels in the diffusion flame. The smoke point is

related to the hydrocarbon type composition of such fuels. Generally, the more

aromatic the fuel the smokier the flame. A high smoke point indicate a fuel of low

smoke producing tendency.

The smoke point (Luminometer number with which it can be correlated) is

quantitatively related to potential radiant heat transfer from the combustion

29
products of the fuel. Because radiant heat transfer exert a strong influence on a

metal temperature of combustor liners and other hot sections of the gas turbine, a

smoke point provide a basis for correlation of fuel characteristic with life of these

component.

Apparatus and materials/Procedure

 Smoke point lamp,

 wick of woven solid circular cotton of ordinary quality,
 Wick tube,
 Candle,
 Sample of kerosene and diesel fuel.

Procedure

 A 126 mm long dried wick is soaked in the sample and placed in the wick tube of

the candle.

 A 10-20 ml of prepared sample is introduced at room temperature into the dry

candle.

 The wick tube is placed in the candle firmly with taking care of the candle air

vent is free from fuel. A new clean, sharp razor is used to cut the wick at the

face of the holder and remove wisps and frayed ends.

 The candle is lighted and the wick adjusted so that the flame is approximately

10 mm high with 5 min.

 After burning, the candle raised until a smoky tail appears, then the candle is

lowered slowly through several stages of flame appear once.

 The maximum height of flame that can be achieved without smoking is

determined to the nearest 0.5 mm.

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 The candle is removed from the lamp rinse with heptane and purged with air to

make ready for re-use. 9.5 Result and Calculations In this experiment we have

to record the height of the flame, when we raise the candle until a smoky tail

appears then lower the flame slowly until the smoky tail disappears, To

eliminate errors due to parallax, the eye of the observer should be slightly to

one side of the centerline, so that a reflected image of the flame is seen on the

scale on one side of the central vertical white line.

2.7.3 POUR POINT TEST (ASTM D97)

The pour point of a liquid is the temperature at which below the liquid loses its

flow characteristics. In crude oil a high pour point is generally associated with a

high paraffin content, typically found in crude deriving from a larger proportion of

plant material.

Fig 2.7.3.0 Pour Point Tester

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Procedure

ASTM D97, Standard Test Method for Pour Point of Crude Oils. The specimen is

cooled inside a cooling bath to allow the formation of paraffin wax crystals. At

about 9 °C above the expected pour point, and for every subsequent 3 °C, the test

jar is removed and tilted to check for surface movement. When the specimen does

not flow when tilted, the jar is held horizontally for 5 sec. If it does not flow, 3 °C

is added to the corresponding temperature and the result is the pour point

temperature.

It is also useful to note that failure to flow at the pour point may also be due to

the effect of viscosity or the previous thermal history of the specimen.

Therefore, the pour point may give a misleading view of the handling properties of

the oil. Additional fluidity tests may also be undertaken. An approximate range of

pour point can be observed from the specimen's upper and lower pour point.

2.7.4 ANILINE POINT TEST (ASTM D611)

The aniline point of an oil is defined as the minimum temperature at which equal

volumes of aniline (C6H5NH2) and the lubricant oil are miscible, i.e. form a single

phase upon mixing. The value gives an approximation for the content of aromatic

compounds in the oil, since the miscibility of aniline, which is also an aromatic

compound, suggests the presence of similar (i.e. aromatic) compounds in the oil.

The lower the aniline point, the greater is the content of aromatic compounds in

the oil.

Determination of aniline point is a test to evaluate base oils that are used in oil

mud. The test indicates if oil is likely to damage elastomers (rubber compounds)

that come in contact with the oil. Aniline point of oil gives an indication of the

32
possible tendency of deterioration of oil when it comes into contact with packing,

rubber sealing etc. in general oils with a high aromatic content are more

detrimental to rubber products than those with a low aromatic content. The

relative aromatic content of an oil is indicated by its aniline point and oils with a

high aromatic content have a low aniline point and vice versa. The higher the aniline

point of the oil, the more desirable it is for drilling fluid usage.

The aniline point serves as a reasonable proxy for aromaticity of oils consisting

mostly of saturated hydrocarbons (i.e. alkanes, paraffins) or unsaturated

compounds (mostly aromatics). Significant chemical functionalization of the oil

(chlorination, sulfonation, etc.) can interfere with the measurement, due to

changes to the solvency of the functionalized oil. The aromatic oil with a

75%aromatic content, the aniline point would be between 32.2° and 48.9°C; for

a naphthenic type containing 40% aromatic structures, it would be between 65.6°

and 76.7°C; and for a paraffinic oil with a15% aromatic content it would be

between 93.3° and 126.7°C.

Fig. 2.7.4.1 Aniline Point Tester

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2.8 HUMAN SAFETY AND ENVIRONMENT (HSE).

Safety is the state of being "safe" (from French sauf), the condition of being

protected from harm or other non-desirable outcomes. Safety can also refer to

the control of recognized hazards in order to achieve an acceptable level of risk .

HSE is a very important entity in NNPC, R&D Division. The training involves the

ways to identify the hazards involved at all the project sites, and employs

necessary preventive measure to avert accidents and fatalities and perform

regular site inspection to ensure that the safety guidelines are adhered to. I was

taught how to ensure that the projects are undergone safely and in compliance

with safety policies which are.

1. High-Risk Situations: Do not start up or shut down equipment or

installations without using the appropriate, written operating procedure.

2. Traffic: Do not exceed the speed limit.

3. Body Mechanics and Tools: Do not carry out work if you do not have the

right tools for the job and the environment.

4. Protective Equipment: Do not access installations or perform work without

wearing general or task-specific PPE.

5. Work Permits: Do not perform work without a valid work permit.

6. Lifting Operations: Do not walk or stand under a load while lifting is taking

place

7. Powered Systems: Do not perform work without checking that the power

and product supply has been rendered in-operative.

8. Confined Spaces: Do not enter a confined space until isolation has been

verified and the atmosphere checked.

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 9. Work at Height: Do not work at height without a safety harness when

there is no collective protective equipment.

10. Change Management: Do not make any technical or organizational

changes without prior authorization.

2.8.1 BASIC FIRE FIGHTING

During this industrial training, we had orientation on basic firefighting by Human

Safety and Environment (H.S.E) Department to help improve our H.S.E awareness.

It was also designed to introduce to us the cause of industrial fire, prevention

principles and fighting techniques. The following are some of the basics taught:

SOURCES OF FIRE

 Mechanical heat energy

 Chemical heat energy

 Solar heat energy

 Electrical heat energy

 Nuclear heat energy

2.8.2 FIRE EXTINGUISHER

A fire extinguisher is an active fire protection device used to extinguish or control

small fires, often in emergency situations. It is not intended for use on an out-of-

control fire, such as one which has reached the ceiling, endangers the user (i.e., no

escape route, smoke, explosion hazard, etc.), or otherwise requires the expertise

of a fire department.

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TYPES OF EXTINGUISHER

 extinguisher that expels water

 extinguisher that expels foam

 extinguisher that expels dry chemical powder

FIRE EXTINGUISHING METHODS

 Cooling: this extinguishment is achieved by temperature reduction or

elimination

 Starvation: this refers to extinguishment by fuel removal

 Smothering: this refers to extinguishment by oxygen dilution

 Flame inhibition: this is extinguishment by flame inhibition

Fire extinguisher can be applied by the PASS method

 P- Pull the pin ; remove the safety pin by pulling the ring

 A- aim the nozzle; energize extinguisher by slightly squeezing the nozzle

 S- squeeze the trigger, this releases the extinguishing agent

 S- sweep from side to side

2.9 SKILLS AND KNOWLEDGE ACQUIRED DURING SIWES PROGRAMME

During my period of industrial attachment NNPC, R&D Division, I had the privilege

to hoard a lot of knowledge, mostly practical and theoretical. The SIWES

programme allowed me the opportunity to put to practice what I’ve been learning

so far as a student in the lecture room. Listed below is a summary of the skills and

knowledge I acquired;

 Knowledge about procedure for crude oil assay

 Whole Crude oil characterization. (I.e.)

i. By D86 Distillation of the crude oil

36
 ii. By Atmospheric distillation (ASTM D2982) Distillation Vacuum

distillation (ASTM D526)

iii. Physico-chemical properties of crude oil and products

iv. Analysis of hydrocarbon fraction/cuts

v. Analysis of the overhead gas (off-gases)

 Fuel blending

 Routine checks.

 Theoretical knowledge on major equipments, devices and instruments that aid

crude refining process, their basic operations, common problems, etc. Also,

tutoring on fire and safety in the chemical plant and measures to respond to any

form of emergency or accident.

CHAPTER THREE

37
 CONCLUSION, PROBLEM ENCOUNTERED AND RECOMMENDATION

3.1 CONCLUSION

The Student Industrial Work Experience Scheme (SIWES) is one of the best

ideas introduced to the university education scheme. Its relevance cannot be over

emphasized. Through the Industrial Training Fund (ITF), the SIWES programme

has shown the importance of the exposure of a student to the Industry, coupled

with the practical knowledge acquired. The programme helps students in several

disciplines of sciences, engineering and technology to experience, learn, practice

and appreciate what they are been taught in their various institutions.

In my Internship with Nigeria National Petroleum Corporation, Research and

Development (R&D) Division, I have acquired a lot of skills related Crude oil Assay

and other auxiliary processes, beyond what I previously known.

The programme has made it possible for me to have of work ethics and to mix up

with other individuals at different levels in their various working place. It exposed

me to unlimited knowledge with regard to activities carried out in my work place.

It is imperative on the part of the Industrial Training Fund (ITF) to put in place

polices to ensure the programme is regulated throughout every tertiary institution

and students benefit from the scheme. As this will go a long way in the boosting of

the Nation’s industry sector for the upcoming young labor force with prior

knowledge of the system, its practice and how to drive the Nation to become self-

sustained and efficient in production.

3.2 PROBLEM ENCOUNTERED

38
  Finding a suitable place for the training with current economic situation of

the country.

 Inadequate communication between ITF area office with deployed SIWES

students to firms.

 Non-payment of monthly salary by firm or ITF to aid the student’s

ongoing SIWES programme.

 No supervision visits paid by ITF officials during Industrial training to

assess and aid the deployed SIWES student

3.3 RECOMMENDATION

My recommendations are:

1. Future participant (student) should try to submit their application to relevant

companies as much as possible before the commencement of the training period.

2. The Industrial Training Fund should partner with firms and organizations in the
country to help post students to firms with ease.

3. Students participating should know that the benefit of any industrial training
can be obtained if they are willing to learn from their supervisor and other
professionals.

4. The ITF should also carry out preliminary visit to the firms to ascertain the
operations and working conditions are favorable for an Industrial Trainee
student.

5. Payments of salaries to deployed students should be made to students during

their Industrial attachment, rather than several months after it had been
concluded.

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